Diisopropylethylamine → 6-(3,5-difluorophenyl)-3-methyl-7-[1-(7H-pyrrolo[2,3-d]pyrimidin-4-ylamino)ethyl]5H-[1,3]thiazolo[3,2-a]pyrimidin-5-one

HRID 58253ノート

反応式

HRID 58253 の反応式
Cl.[NH2:2][CH:3]([C:5]1[N:6]=[C:7]2[S:22][CH:21]=[C:20]([CH3:23])[N:8]2[C:9](=[O:19])[C:10]=1[C:11]1[CH:16]=[C:15]([F:17])[CH:14]=[C:13]([F:18])[CH:12]=1)[CH3:4].Cl[C:25]1[N:30]=[CH:29][NH:28][C:27]2=[N:31][CH:32]=[CH:33][C:26]=12.C(N(CC)C(C)C)(C)C>C(O)(C)C>[F:18][C:13]1[CH:12]=[C:11]([C:10]2[C:9](=[O:19])[N:8]3[C:20]([CH3:23])=[CH:21][S:22][C:7]3=[N:6][C:5]=2[CH:3]([NH:2][C:25]2[C:26]3[CH:33]=[CH:32][NH:31][C:27]=3[N:28]=[CH:29][N:30]=2)[CH3:4])[CH:16]=[C:15]([F:17])[CH:14]=1

参加物

5

反応物 3

HCID 81531DiisopropylethylamineHCID 668644077-(1-aminoethyl)-6-(3,5-difluorophenyl)-3-methyl-5H-[1,3]thiazolo[3,2-a]pyrimidin-5-one hydrochlorideHCID 178418725HCID 178418725、化合物

生成物 1

HCID 509959086-(3,5-difluorophenyl)-3-methyl-7-[1-(7H-pyrrolo[2,3-d]pyrimidin-4-ylamino)ethyl]5H-[1,3]thiazolo[3,2-a]pyrimidin-5-one

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

反応条件

温度
100 °C

実験手順

A mixture of 7-(1-aminoethyl)-6-(3,5-difluorophenyl)-3-methyl-5H-[1,3]thiazolo[3,2-a]pyrimidin-5-one hydrochloride (0.030 g, 0.084 mmol), 4-chloropyrrolo[2,3-d]pyrimidine (0.013 g, 0.084 mmol), and N, N-diisopropylethylamine (0.044 mL, 0.25 mmol) in isopropyl alcohol (0.2 mL) was heated at 100° C., in a sealed tube, for three days. The resultant mixture was applied on RP-HPLC (XBridge C18 Column, eluting with a gradient of acetonitrile/water containing 0.15% NH4OH) to give the desired product. LCMS calculated for C21H17F2N6OS (M+H)+: m/z=439.1. Found: 439.1.

後処理

  1. washeluting with a gradient of acetonitrile/water containing 0.15% NH4OH)

出典と根拠

ORDレコード
ord-77063e3a58b84c19a58efd6effb1b887
出典データセット
uspto-grants-2016_09
特許番号
US09434746B2

反応ノート

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